School of Environmental Science and Engineering, Suzhou University of Science and Technology, No. 1 Kerui Road, Suzhou, 215009, PR China.
School of Environmental Science and Engineering, Suzhou University of Science and Technology, No. 1 Kerui Road, Suzhou, 215009, PR China; Jiangsu Key Laboratory of Environmental Science and Engineering, Suzhou University of Science and Technology, No. 1 Kerui Road, Suzhou, 215009, PR China.
Ecotoxicol Environ Saf. 2019 Jul 30;176:20-26. doi: 10.1016/j.ecoenv.2019.03.063. Epub 2019 Apr 1.
Microcystins is a class of monocyclic of heptapeptides with many different isomerides. It has become potential hazardous material in water environment for its toxic, distribution and stability. This project worked on a method for determination of trace microcystin (MC-LR and MC-RR) in environmental waters. The ionic liquid magnetic graphene (IL@MG) was prepared and applied to the concentration and determination of microcystins, based on magnetic solid phase extraction (MSPE), and coupled with ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The ionic liquid magnetic graphene was prepared by coprecipitatial synthesis and characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), fourier transform infrared spectroscopy (FT-IR), specific surface area (BET), pore size distribution (BJH) and magnetic hysteresis loop. The experimental parameters of magnetic solid phase extraction, including amount of IL@MG, pH, extraction time and elution solvent were investigated by a univariate method and orthogonal screening. The method showed good linearity in the range of 0.01-10.0 g/L and 0.005-10.0 μg/L for MC-LR and MC-RR, when the pH of water samples was 4.00 and 10.0 mg adsorbents were used to extract targets for 18 min. The lowest detection limit was 0.414 ng/L and 0.216 ng/L for MC-LR and MC-RR respectively. The recoveries of the microcystins were in the range of 83.6-100.9%, and the relative standard deviation was less than 7.59%. The trace amount of MC-LR (0.020 μg/L) and MC-RR (0.003 μg/L and 0.021 μg/L) was detected in actural water samples. Attributed to its simple operator, low detection limit and high sensitivity, this method could be used for the detection of trace microcystins in water samples.
微囊藻毒素是一类具有多种同分异构体的单环七肽。由于其毒性、分布和稳定性,已成为水环境中的潜在危险物质。本项目研究了一种测定环境水中痕量微囊藻毒素(MC-LR 和 MC-RR)的方法。基于磁固相萃取(MSPE),制备了离子液体磁性石墨烯(IL@MG),并将其与超高效液相色谱-串联质谱(UHPLC-MS/MS)联用,用于微囊藻毒素的浓缩和测定。采用共沉淀合成法制备了离子液体磁性石墨烯,并通过扫描电子显微镜(SEM)、透射电子显微镜(TEM)、傅里叶变换红外光谱(FT-IR)、比表面积(BET)、孔径分布(BJH)和磁滞回线对其进行了表征。通过单因素法和正交筛选法考察了磁固相萃取的实验参数,包括 IL@MG 的用量、pH 值、萃取时间和洗脱溶剂。当水样的 pH 值为 4.00 且使用 10.0 mg 吸附剂提取目标物 18 min 时,MC-LR 和 MC-RR 的线性范围分别为 0.01-10.0 g/L 和 0.005-10.0 μg/L。MC-LR 和 MC-RR 的最低检测限分别为 0.414 ng/L 和 0.216 ng/L。微囊藻毒素的回收率在 83.6%-100.9%之间,相对标准偏差小于 7.59%。在实际水样中检测到痕量的 MC-LR(0.020 μg/L)和 MC-RR(0.003 μg/L 和 0.021 μg/L)。由于其操作简单、检测限低、灵敏度高,该方法可用于水样中痕量微囊藻毒素的检测。